CN104098996B - A kind of nano compound polyurethane aircraft coating and preparation method thereof - Google Patents
A kind of nano compound polyurethane aircraft coating and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to nanotechnology and corrosion protection technology, be specially a kind of nano compound polyurethane aircraft coating with high corrosion-resistant and preparation method thereof.Count by weight, component one is made up of water based acrylic resin 60-80 part, nano slurry 5-10 part, coloring pigment 1-3 part, organic inhibitor 8-10 part, rust resisting pigment 10-15 part etc., and component two is made up of water-based isocyanate firming agent 70-80 part, deionized water 20-30 part.The raw materials such as polyurethane aircraft coating, deionized water, nano slurry, auxiliary agent being carried out high speed dispersion, then grinds, make component one after filtering, with deionized water dispersion, firming agent is mixed and made into component two, two components Homogeneous phase mixing in proportion obtains coating.Adopt Novel composite nano slurry, rust resisting pigment, compound organic inhibitor and water etc. to prepare nano compound polyurethane aircraft coating so that nano-powder material stably dispersing in coating, and improve the corrosion resistance of coating.
Description
Technical field
The present invention relates to nanotechnology and corrosion protection technology, be specially a kind of nano compound polyurethane paint with high corrosion-resistant and preparation method thereof.
Background technology
Aircraft coating, for covering with paint and the protection of aircraft skin, is not only the decorative appearance material of aircraft, but also is the important materials of the aircaft configuration extending aircraft utilization life-span, guarantee safe flight.Department of CAAC once predicted, within 2011, domestic big aircraft C919 will welcome new order, at present the order of existing 100 framves, and following 20 years total sales volumes will reach 2000 framves；Need all kinds of general and military aviation aircraft more than 10,000 framves to China in 2012, newly make and keep in repair required various aircraft coatings and be up to 5000 tons, high performance aircraft coating is had very big demand.Existing aircraft coating, including a nanometer aircraft coating, in performances such as decoration, anticorrosion, antifouling, self-cleaning property, uvioresistant, Defend salt fog, wet-heat resisting and low frictions and in service life, there is a portion effect, but over-all properties qualified can not reached；It is generally 6-9 especially with the life-span.
Used airplane dope is mainly made up of epoxy or polyurethane primer and polyurethane finish.The function of aviation priming paint is a lot of, most important of which is that and prevents matrix corrosion.Moisture in atmospheric environment, oxygen, salt fog, acid mist and machine liquid etc. are the principal elements causing corrosion.Owing to common coating has certain permeability for Korrosionsmedium, it is inadequate for therefore only protecting by finish paint.The effect of priming paint is then on the basis of bottom paint resin, is slowed down the infiltration of Korrosionsmedium by the compactness of filler pigment increasing subbing, relies on the physics of rust resisting pigment and chemical action to stop material property to worsen.At present, the chromate such as strontium chromate, zinc chromate, barium chromate is main rust resisting pigment in aircraft priming paint, and consumption is typically in the 10wt%-20wt% of priming paint total amount.As Chinese patent (publication number CN1891770) discloses aircraft skin coating, priming paint adopts intermediate molecular weight epoxy resin to arrange in pairs or groups mutually with relatively soft polyamide curing agent, finish paint adopts special hydroxy polyester resin to arrange in pairs or groups mutually with HDI biuret and the HDI trimer as cross-linking agent, contains the strontium chromate of 13wt%-14wt% in the base material of priming paint.Chromate is poisonous, carcinogenic material, in industrial processes, health and environment is worked the mischief.The decree that restriction chromate uses is put into effect in all trades and professions successively, and the aircraft coating of Devoting Major Efforts To Developing Chrome-free is inexorable trend.
Bicomponent polyurethane coating is due to energy normal temperature cure, and paint film has the advantages such as chemical proof, wearability, freeze-thaw resistance, good weatherability, it has also become the leading products of aircraft coating.There are high performance polyurethanes aircraft coating in the countries such as the U.S., Holland, Germany.Finch paint chemistry company, Steling spray paint company, U.S.'s paint company, AKZO company of Holland and DESOTO company of Britain all production and selling polyurethanes aircraft coatings.In 1976, US Patent No. P3,989,676 just reported the polyepoxide-caprolactone polyol that can be used for aircraft outer surface and polyisocyanate prepares polyurethane coating.US Patent No. P4,110,317 report the polyurethane coating being made up of isocyanate-terminated prepolymer etc., can be used for the weatherability of helicopter blade, radome etc. and erosion resistant protection.US Patent No. P4,155,896 report the conductive polyurethane coating containing metallic fiber suitable in aircaft configuration, can carry out lightning protected or eliminate electrostatic.But medium-sized aliphatic polyurethane top coat is main coat system, due to gloss retention and colour retention not enough, after using two, three years, the gloss of coating constantly declines, and has lost original gloss by about 5 years, it is run ragged in appearance, also commercial competitiveness [what tripod, Lei Junzhi, Hua Xinhao are just lost, aircraft coating and application techniques, Chemical Industry Press, 2000, P175].Existing aliphatic polyurethane top coat increases by one layer of ultraviolet light varnish, although gloss retention and colour retention improve, but add one working procedure, too increase man-hour and cost.
Summary of the invention
It is an object of the invention to provide nano compound polyurethane aircraft coating of a kind of high anti-corrosive properties, high-durability, high soil resistance, high surface self-cleaning, high anti-UV and long service life and preparation method thereof, solve prior art aircraft coating adopts material poisonous, harmful, to problems such as health and environment work the mischief.
The technical scheme is that
A kind of nano compound polyurethane aircraft coating, is made up of component one and component two, wherein:
(1) counting by weight, component one is made up of following components and content:
Water based acrylic resin 60-80 part；
Nano slurry 5-10 part；Nano slurry is made up of nano titanium oxide, nano silicon, deionized water, silane coupler, PAMC dispersant and waterborne polyurethane resin, wherein: nano titanium oxide, nano silicon, deionized water weight ratio be (10～20): (40～50): (30～50), silane coupler accounts for the 2～4% of above-mentioned nanoparticle gross weight, polyacrylamide dispersant accounts for the 3～5% of above-mentioned nanoparticle gross weight, waterborne polyurethane resin accounts for the 5～8% of above-mentioned nanoparticle gross weight；
Coloring pigment 1-3 part；
Organic inhibitor 8-10 part, organic inhibitor is the compositions of laruate, palmitate, stearate and cinnamate；
Rust resisting pigment 10-15 part, rust resisting pigment is polyaniline modified micaceous iron oxide or polyaniline-modified glass flakes；
Filler 1-5 part；
Auxiliary agent 1-3 part；
Deionized water 20-30 part；
(2) counting by weight, component two is made up of following components and content:
Water-based isocyanate firming agent 70-80 part；
Deionized water 20-30 part；
The weight proportion of component one and component two is (100:10)～(100:30).
Described nano compound polyurethane aircraft coating, laruate be sodium laurate, potassium laurate one or both, palmitate be sodium palmitate, potassium palmitate one or both, stearate be sodium stearate, potassium stearate one or both, cinnamate be Fortificar, potassium cinnamate one or both.
Described nano compound polyurethane aircraft coating, the structure of polyaniline modified micaceous iron oxide is laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is micaceous iron oxide；The thickness of clad is 10～20 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 80～90wt%, and phytic acid accounts for 10～20wt%.
Described nano compound polyurethane aircraft coating, the structure of polyaniline-modified glass flakes, for being laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is glass flake；The thickness of clad is 10～30 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 80～90wt%, and phytic acid accounts for 10～20wt%.
The preparation method of described nano compound polyurethane aircraft coating, as follows operation:
1) water based acrylic resin, deionized water, nano slurry, auxiliary agent are added in a reservoir, high speed dispersor is utilized to disperse 5～10 minutes at 400～500rpm, add coloring pigment, organic inhibitor, rust resisting pigment and filler, disperse 20～30 minutes through 500～1000rpm；
2) above-mentioned material being carried out sand milling, the sand milling time is 1～4 hour, behind test fineness≤40 μm, and discharging, filter, packaging, prepare into component one；
3) water-based isocyanate firming agent is joined in stirred tank, add deionized water dilution, utilize high speed dispersor to disperse 5～20 minutes at 400～500rpm, discharging after filtration, packaging, prepare into component two；
4) adding in component one by component two, after stirring, spraying, brushing or dip-coating are in substrate surface, room temperature or the formation nano compound polyurethane aviation coating that is heating and curing.
The preparation method of described nano compound polyurethane aircraft coating, when rust resisting pigment is polyaniline modified micaceous iron oxide, the preparation method of polyaniline modified micaceous iron oxide is as follows:
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein, phosphoric acid is 0.01～5 mol/L, and phytic acid is 0.01～1 mol/L；
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.01～1 mol/L, continues to stir；Take phosphoric acid and phytic acid, aniline mixed aqueous solution 500ml, add 200～1000 order micaceous iron oxides of 5～1000g, and after stirring, be pre-chilled to 0～10 DEG C；
The aqueous solution of (c) preparation oxidant: in solution, the concentration of oxidant is 0.05～5 mol/L, and the aqueous solution of oxidant is pre-chilled to 0～10 DEG C；Oxidant is one or more mixture of Ammonium persulfate., hydrogen peroxide, potassium peroxydisulfate, benzoyl peroxide；
D solution prepared for 500ml step (c) is add containing in the phosphoric acid prepared for 500ml step (b) of micaceous iron oxide and phytic acid, aniline mixed aqueous solution in 10～30 minutes in the time by (), react 1～8 hour at 0～10 DEG C, centrifugal, with distilled water wash, 80～100 DEG C after dry 1～5 hour, with mortar grinder, and sieve, obtain the micaceous iron oxide that bottle-green 200～1000 order electrically conductive polyanilines are modified.
The preparation method of described nano compound polyurethane aircraft coating, when rust resisting pigment is polyaniline-modified glass flakes, the preparation method of polyaniline-modified glass flakes is as follows:
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein phosphoric acid is 0.01～5 mol/L, and phytic acid is 0.01～1 mol/L；
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.01～1 mol/L, continue to stir, take phosphoric acid and phytic acid, aniline mixed aqueous solution 500ml, add the 80-1000 order glass flake of 5～1000g, and stir, it is pre-chilled to 0～10 DEG C；
The aqueous solution of (c) preparation oxidant: in solution, the concentration of oxidant is 0.05～5 mol/L, and the aqueous solution of oxidant is pre-chilled to 0～10 DEG C；Oxidant is one or more mixture of Ammonium persulfate., hydrogen peroxide, potassium peroxydisulfate, benzoyl peroxide, ferric chloride, potassium dichromate, potassium permanganate；
(d) by solution prepared for 500ml step (c) the time be add in 10～30 minutes step (b) prepared containing in the 500ml phosphoric acid of glass flake and phytic acid, aniline mixed aqueous solution, react 1～8 hour at 0～10 DEG C, centrifugal, with distilled water wash, 80～100 DEG C after dry 1～5 hour, with mortar grinder, and sieve, obtain the glass flake that bottle-green 80～1000 order electrically conductive polyanilines process.
The preparation method of described nano compound polyurethane aircraft coating, the preparation method of nano slurry is as follows:
Nano titanium oxide and nano silicon are added in deionized water, carries out ultrasound wave and disperse 20～30 minutes, temperature T=30～40 DEG C；It is separately added into silane coupler, PAMC dispersant and waterborne polyurethane resin more wherein and carries out ultrasound wave dispersion 1～2 hour, temperature T=50～60 DEG C；Last in (1～3) × 104It is centrifuged 2～3 times under rev/min, centrifugal 0.5～2 hour every time, prepares nano slurry.
The design philosophy of the present invention is:
(1) nano slurry
Nano slurry is uniformly mixed by nano titanium oxide, nano silicon, water, silane coupler, PAMC dispersant, waterborne polyurethane resin, by modifying agent such as silane coupler, PAMC dispersant, waterborne polyurethane resins to nano particle surface modifying, to improve its compatibility, and compatible with selected coating system.Wherein:
PAMC dispersant (PAM) is chain macromolecule compound, owing to it has multiple active group, and can, absorption formation hydrogen bond affine with many materials.Owing to PAM strand containing carboxyl, there is the capillary effect of reduction, contribute to water moistening solid, this is advantageous particularly for nanoparticle dispersion in water, when PAM adds slurry, it is possible to make nanoparticle surface form bimolecular structure, outer layer dispersant is extreme and water has stronger affinity, add the degree that nanoparticle is spontaneously wet out by water, between solid particle because of electrostatic repulsion away from, reach good dispersion effect.
Silane coupler is as binding agent and surface conditioning agent, and silane coupler can improve the bond properties of waterborne polyurethane resin, and the action principle as viscosifier is in that itself has two kinds of groups: a kind of group can combine with the framework material glued；Another kind of group then can be combined with PAMC dispersant or waterborne polyurethane resin, thus forming powerful higher chemical bond at bonding interface, substantially improves adhesive strength.
Waterborne polyurethane resin is mainly used in promoting the adherence of nano slurry, has the ultra-fine thin film causing and extending, excellent tolerance to cold, but will not grain excessively be filled.
(2) organic inhibitor
Organic inhibitor is the compositions of laruate, palmitate, stearate and cinnamate, wherein:
The sodium laurate of abluent, insecticide and pharmaceuticals industry and potassium laurate are used for organic inhibitor, there is high anti-corrosive properties, high-durability, and environment-protecting asepsis is harmless.
The sodium palmitate of pharmaceuticals industry and potassium palmitate are used for organic inhibitor, there is high soil resistance, high surface self-cleaning, high anti-UV, and environment-protecting asepsis is harmless.
The sodium stearate of metal heat treatmet and stabilizer for plastics and potassium stearate are used for organic inhibitor, there is the effect improving coating activity, floating voltinism and stability, and environment-protecting asepsis is harmless.
The Fortificar of pharmaceuticals industry, potassium cinnamate are used for organic inhibitor, there is the effect of sterilization and anticorrosion and antioxygen, and environment-protecting asepsis is harmless.
(3) rust resisting pigment
Rust resisting pigment is polyaniline modified micaceous iron oxide or polyaniline-modified glass flakes, wherein:
Polyaniline modified micaceous iron oxide can realize passivation and the inhibition of metal base, improve corrosion resistance and the permeability resistance of conventional MIO coating, can replacing the leaded and chromate pigment in conventional MIO coating, prepared coating meets the environmental requirement without harmful pigment.Utilizing oxidative polymerization method to form the clad of polyaniline and phytic acid on micaceous iron oxide surface, metal is had passivation and corrosion inhibition by the micaceous iron oxide after process.
Polyaniline-modified glass flakes can realize passivation and the inhibition of metal base, improves corrosion resistance and the permeability resistance of Conventional glass flake paint.Utilizing oxidative polymerization method to form polyaniline-coated layer on glass flake surface, metal is had passivation by the glass flake after process, and metal is also functioned to the effect of inhibition by the phytic acid clad on glass flake surface.
In the present invention, organic inhibitor and rust resisting pigment match, and rust resisting pigment can form protecting film at coating and metal interface after dissolution in water, plays corrosion-resisting function.Sudden strain of a muscle rust when organic inhibitor can resist due to coating application occurs, and has used collaborative corrosion-resisting function together with rust resisting pigment.
In the present invention, coloring pigment is coating common pigments, as: titanium dioxide, zinc oxide or Griffith's zinc white. etc..
In the present invention, filler is coating customary filler, as: GL ground limestone, precipitated calcium carbonate, Pulvis Talci or quartz sand etc..
In the present invention, auxiliary agent is auxiliary agent commonly used in dope preparing process, including anti-settling agent, wetting dispersing agent or levelling agent etc..
Advantages of the present invention and having the beneficial effect that:
1, the compositions that organic inhibitor is laruate, palmitate, stearate and cinnamate of nano compound polyurethane aircraft coating of the present invention, has the features such as high anti-corrosive properties, high-durability, high soil resistance, high surface self-cleaning, high anti-UV and long service life.
2, nano compound polyurethane aircraft coating of the present invention adopts rust resisting pigment to be polyaniline modified micaceous iron oxide or polyaniline-modified glass flakes, and rust resisting pigment used is nontoxic, is conducive to environmental protection.
3, nano compound polyurethane aircraft coating of the present invention due to adopt composite nano slurry, rust resisting pigment, compound organic inhibitor and water compound use formed water-based polyurethane aircraft coating by so that the permeability resistance of coating, corrosion resistance significantly improve.
4, nano compound polyurethane aircraft coating of the present invention has excellent storage stability, the feature such as not easily sinks to the bottom.
5, nano compound polyurethane aircraft coating of the present invention has substrate surface treatment requirement is low and metal base adhesion strong, and the advantage that matching is good, antiseptic property is good is stablized in storage.
Detailed description of the invention
In the present invention unless specifically stated otherwise outside, involved ratio is weight ratio.
Preparation method of sample: some 150mm × 75mm × 2mmLY12 aluminium alloy plate surface is after oil removal treatment, spraying twice coating (build is 40 ± 5 μm), coating is respectively adopted the polyurethane coating of nano compound polyurethane aircraft coating, contrast, after normal temperature drying 7 days, carry out coating performance test.
Performance evaluation: the neutral salt spray test of coating sample adopts the ST-ISO-3 salt mist tester of Japan Xu He testing machine Co., Ltd..NaCl solution concentration is 3.5wt%, and test temperature is 40 ± 2 DEG C, continuously spraying 1500 hours, and neutral salt spray test performs standard GB1771-79, evaluates coating salt fog resistance grade according to GB1740-79.
Below, by embodiment, the present invention is described in more detail.
Embodiment 1
1, the preparation of nano slurry
By nano titanium oxide, nano silicon, water weight ratio be 15:45:40, nano titanium oxide and nano silicon are added deionized water for ultrasonic ripple (temperature T=40 DEG C) dispersion 20min；Addition accounts for the silane coupler of above-mentioned nanoparticle gross weight 3%, accounts for the polyacrylamide dispersant of above-mentioned nanoparticle gross weight 4% and account for the waterborne polyurethane resin of above-mentioned nanoparticle gross weight 6% wherein again, carries out ultrasound wave (T=55 DEG C) dispersion 1h；Last 2 × 104Being centrifuged 3 times under rev/min, centrifugal 1h, prepares nano slurry every time.
2, the preparation of polyaniline modified micaceous iron oxide
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein phosphoric acid is 1.5 mol/L；Phytic acid is 0.5 mol/L.
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.5 mol/L.Continue stirring 0.5 hour.Take phosphoric acid and phytic acid, aniline mixed aqueous solution 500ml, add the 325 order micaceous iron oxides of 70g, and after stirring 10 minutes, be pre-chilled to 8 DEG C.
The aqueous solution of (c) preparation oxidant: selecting benzoyl peroxide as oxidant, the concentration of preparation benzoyl peroxide is 1.5 mol/L.The aqueous solution of benzoyl peroxide is pre-chilled to 8 DEG C.
D (c) 500ml solution was slowly added in the 500ml phosphoric acid containing micaceous iron oxide and phytic acid, aniline mixed aqueous solution (b) by () in 10～30 minutes, react 3 hours at 5 DEG C, centrifugal, with distilled water wash, 90 DEG C after dry 2 hours, with mortar grinder, after screening, obtain the micaceous iron oxide that bottle-green 325 order electrically conductive polyanilines are modified.The structure of obtained polyaniline modified micaceous iron oxide is laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is micaceous iron oxide；The coating thickness of the present embodiment is 20 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 80wt%, and phytic acid accounts for 20wt%.
3, the preparation of component one
Dispersion cylinder adds 70kg water based acrylic resin, add deionized water 25kg, it is subsequently adding above-mentioned nano slurry 8kg, add BYK-P104S wetting dispersing agent 0.8kg, BYK-310 levelling agent 0.2kg, BENTONE34 organobentonite anti-settling agent (RHEOX company of the U.S.) 0.5kg, high speed dispersor is utilized to disperse 10 minutes at 400rpm, add titanium dioxide 2kg, above-mentioned polyaniline modified micaceous iron oxide 12kg, sodium laurate 2kg, sodium palmitate 2kg, sodium stearate 2kg, Fortificar 2kg, Pulvis Talci 3kg, disperse 20 minutes with high speed dispersor 500rpm；Then grind 2 hours with horizontal sand mill, after being 25 microns to fineness, filter, pack, prepare into the component one of nano compound polyurethane aircraft coating.
4, the preparation of component two
Water-based isocyanate firming agent is mixed homogeneously in addition dispersion cylinder by weight 80:20 with deionized water, filters after disperseing 10 minutes with high speed dispersor 500rpm, pack.
Two components are by component one: make nano compound polyurethane aircraft coating after the stirring of component two=5:1 (weight ratio) proportioning.Spraying this nano compound polyurethane aircraft coating on the LY12 aluminium alloy of 75mm × 150mm × 2mm, dry 7 days under room temperature, build is 40 ± 5 μm.
Embodiment 2
1, the preparation of nano slurry
By nano titanium oxide, nano silicon, water weight ratio be 10:50:40, nano titanium oxide and nano silicon are added deionized water for ultrasonic ripple (temperature T=30 DEG C) dispersion 30min；Addition accounts for the silane coupler of above-mentioned nanoparticle gross weight 2%, accounts for the polyacrylamide dispersant of above-mentioned nanoparticle gross weight 5% and account for the waterborne polyurethane resin of above-mentioned nanoparticle gross weight 8% wherein again, carries out ultrasound wave (T=50 DEG C) dispersion 2h；Last 1 × 104Being centrifuged 2 times under rev/min, centrifugal 2h, prepares nano slurry every time.
2, the preparation of polyaniline modified micaceous iron oxide
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein phosphoric acid is 0.5 mol/L；Phytic acid is 0.1 mol/L.
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.1 mol/L.Continue stirring 1.5 hours.Take phosphoric acid and phytic acid, aniline mixed aqueous solution 500ml, add the 325 order micaceous iron oxides of 20g, and after stirring 25 minutes, be pre-chilled to 2 DEG C.
The aqueous solution of (c) preparation oxidant: selecting Ammonium persulfate. as oxidant, the concentration of preparation Ammonium persulfate. is 0.5 mol/L.The aqueous solution of Ammonium persulfate. is pre-chilled to 2 DEG C.
D (c) 500ml solution was slowly added in the 500ml phosphoric acid containing micaceous iron oxide and phytic acid, aniline mixed aqueous solution (b) by () in 10～30 minutes, react 1 hour at 2 DEG C, centrifugal, with distilled water wash, 80 DEG C after dry 5 hours, with mortar grinder, after screening, obtain the micaceous iron oxide that bottle-green 325 order electrically conductive polyanilines are modified.The structure of obtained polyaniline modified micaceous iron oxide is laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is micaceous iron oxide；The coating thickness of the present embodiment is 10 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 90wt%, and phytic acid accounts for 10wt%.
3, the preparation of component one
Dispersion cylinder adds 75kg water based acrylic resin, add deionized water 23kg, it is subsequently adding above-mentioned nano slurry 6kg, add BYK-P104S wetting dispersing agent 0.5kg, BYK-310 levelling agent 0.5kg, BENTONE34 organobentonite anti-settling agent (RHEOX company of the U.S.) 1.0kg, high speed dispersor is utilized to disperse 5 minutes at 500rpm, add titanium dioxide 2.5kg, above-mentioned polyaniline modified micaceous iron oxide 13kg, sodium laurate 2.5kg, sodium palmitate 2kg, sodium stearate 2.5kg, Fortificar 2kg, Pulvis Talci 4kg, disperse 25 minutes with high speed dispersor 800rpm；Then grind 3 hours with horizontal sand mill, after being 25 microns to fineness, filter, pack, prepare into the component one of nano compound polyurethane aircraft coating.
4, the preparation of component two
Water-based isocyanate firming agent is mixed homogeneously in addition dispersion cylinder by weight 70:30 with deionized water, filters after disperseing 20 minutes with high speed dispersor 400rpm, pack.
Two components are by component one: make nano compound polyurethane aircraft coating after the stirring of component two=10:1 (weight ratio) proportioning.Spraying this nano compound polyurethane aircraft coating on the LY12 aluminium alloy of 75mm × 150mm × 2mm, dry 7 days under room temperature, build is 40 ± 5 μm.
Embodiment 3
1, the preparation of nano slurry
By nano titanium oxide, nano silicon, water weight ratio be 20:45:35, nano titanium oxide and nano silicon are added deionized water for ultrasonic ripple (temperature T=35 DEG C) dispersion 25min；Addition accounts for the silane coupler of above-mentioned nanoparticle gross weight 4%, accounts for the polyacrylamide dispersant of above-mentioned nanoparticle gross weight 3% and account for the waterborne polyurethane resin of above-mentioned nanoparticle gross weight 5% wherein again, carries out ultrasound wave (T=60 DEG C) dispersion 1.5h；Last 3 × 104Being centrifuged 3 times under rev/min, centrifugal 0.5h, prepares nano slurry every time.
2, the preparation of polyaniline-modified glass flakes
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein phosphoric acid is 1.2 mol/L；Phytic acid is 0.6 mol/L.
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.5 mol/L.Continue stirring 1.5 hours.Take phosphoric acid and phytic acid, aniline mixed aqueous solution 500ml, add the 240 order glass flakes of 500g, and stir 30 minutes, be pre-chilled to 8 DEG C.
The aqueous solution of (c) preparation oxidant: selecting benzoyl peroxide as oxidant, the concentration of preparation benzoyl peroxide is 1.2 mol/L.The aqueous solution of benzoyl peroxide is pre-chilled to 8 DEG C.
D (c) 500ml solution was slowly added in the 500ml acid containing glass flake and phytic acid, aniline mixed aqueous solution (b) by () in 10～30 minutes, react 3 hours at 5 DEG C, centrifugal, with distilled water wash, 80 DEG C after dry 3 hours, with mortar grinder, after screening, obtain the glass flake that bottle-green 240 order electrically conductive polyanilines are modified.In the present embodiment, the structure of obtained polyaniline-modified glass flakes is laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is glass flake；The coating thickness of the present embodiment is 30 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 80wt%, and phytic acid accounts for 20wt%.
3, the preparation of component one
Dispersion cylinder adds 60kg water based acrylic resin, add deionized water 20kg, it is subsequently adding above-mentioned nano slurry 5kg, add BYK-P104S wetting dispersing agent 0.2kg, BYK-310 levelling agent 0.3kg, BENTONE34 organobentonite anti-settling agent (RHEOX company of the U.S.) 0.5kg, high speed dispersor is utilized to disperse 8 minutes at 450rpm, add titanium dioxide 1kg, above-mentioned polyaniline-modified glass flakes 10kg, potassium laurate 2kg, potassium palmitate 2.5kg, potassium stearate 2kg, potassium cinnamate 2.5kg, Pulvis Talci 1kg, disperse 20 minutes with high speed dispersor 900rpm；Then grind 1 hour with horizontal sand mill, after being 25 microns to fineness, filter, pack, prepare into the component one of nano compound polyurethane aircraft coating.
4, the preparation of component two
Water-based isocyanate firming agent is mixed homogeneously in addition dispersion cylinder by weight 75:25 with deionized water, filters after disperseing 5 minutes with high speed dispersor 500rpm, pack.
Two components are by component one: make nano compound polyurethane aircraft coating after the stirring of component two=10:3 (weight ratio) proportioning.Spraying this nano compound polyurethane aircraft coating on the LY12 aluminium alloy of 75mm × 150mm × 2mm, dry 7 days under room temperature, build is 40 ± 5 μm.
Embodiment 4
1, the preparation of nano slurry
By nano titanium oxide, nano silicon, water weight ratio be 20:45:35, nano titanium oxide and nano silicon are added deionized water for ultrasonic ripple (temperature T=35 DEG C) dispersion 25min；Addition accounts for the silane coupler of above-mentioned nanoparticle gross weight 4%, accounts for the polyacrylamide dispersant of above-mentioned nanoparticle gross weight 3% and account for the waterborne polyurethane resin of above-mentioned nanoparticle gross weight 5% wherein again, carries out ultrasound wave (T=60 DEG C) dispersion 1.5h；Last 3 × 104Being centrifuged 3 times under rev/min, centrifugal 0.5h, prepares nano slurry every time.
2, the preparation of polyaniline-modified glass flakes
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein phosphoric acid is 0.4 mol/L；Phytic acid is 0.1 mol/L.
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.1 mol/L.Continue stirring 1 hour.Take phosphoric acid and phytic acid, aniline mixed aqueous solution 500ml, add the 325 order glass flakes of 200g, and stir 20 minutes, be pre-chilled to 2 DEG C.
The aqueous solution of (c) preparation oxidant: selecting Ammonium persulfate. as oxidant, the concentration of preparation Ammonium persulfate. is 0.5 mol/L.The aqueous solution of Ammonium persulfate. is pre-chilled to 2 DEG C.
D (c) 500ml solution was slowly added in the 500ml acid containing glass flake and phytic acid, aniline mixed aqueous solution (b) by () in 20 minutes, react 1 hour at 2 DEG C, centrifugal, with distilled water wash, 100 DEG C after dry 1 hour, with mortar grinder, after screening, obtain the glass flake that bottle-green 325 order electrically conductive polyanilines are modified.In the present embodiment, the structure of obtained polyaniline-modified glass flakes is laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is glass flake；The coating thickness of the present embodiment is 15 μm, and polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 90wt%, and phytic acid accounts for 10wt%.
3, the preparation of component one
Dispersion cylinder adds 80kg water based acrylic resin, add deionized water 30kg, it is subsequently adding above-mentioned nano slurry 10kg, add BYK-P104S wetting dispersing agent 1.0kg, BYK-310 levelling agent 0.5kg, BENTONE34 organobentonite anti-settling agent (RHEOX company of the U.S.) 0.5kg, high speed dispersor is utilized to disperse 5 minutes at 500rpm, add titanium dioxide 3kg, above-mentioned polyaniline-modified glass flakes 15kg, potassium laurate 2kg, potassium palmitate 2kg, potassium stearate 2kg, potassium cinnamate 2kg, Pulvis Talci 5kg, disperse 20 minutes with high speed dispersor 1000rpm；Then grind 4 hours with horizontal sand mill, after being 25 microns to fineness, filter, pack, prepare into the component one of nano compound polyurethane aircraft coating.
4, the preparation of component two
Water-based isocyanate firming agent is mixed homogeneously in addition dispersion cylinder by weight 80:20 with deionized water, filters after disperseing 15 minutes with high speed dispersor 400rpm, pack.
Two components are by component one: make nano compound polyurethane aircraft coating after the stirring of component two=4:1 (weight ratio) proportioning.Spraying this nano compound polyurethane aircraft coating on the LY12 aluminium alloy of 75mm × 150mm × 2mm, dry 7 days under room temperature, build is 40 ± 5 μm.
Comparative example 1
The preparation method of component one: add 40kg Hydroxylated acrylic resin in dispersion cylinder(solid content is 65wt% to A265, the hydroxy radical content of hard resin is 3.4wt%), add dimethylbenzene 19kg, it is subsequently adding BYK-P104S wetting dispersing agent 0.8kg, BYK-310 levelling agent 0.2kg, BENTONE34 organobentonite anti-settling agent (RHEOX company of the U.S.) 0.5kg, high speed dispersor is utilized to disperse 10 minutes at 400rpm, add titanium dioxide 16kg, Pulvis Talci 23.5kg, disperse 20 minutes with high speed dispersor 500rpm, then grind 2 hours with horizontal sand mill, after being 25 microns to fineness, filter, packaging, prepare the component one of polyurethane coating.
The preparation method of component two: firming agent 80kgN75 (solid content is 75wt%, and NCO content is 16.5wt%) adds in dispersion cylinder, adds 20kg butyl acetate, filters, packs after disperseing 15 minutes with high speed dispersor 500rpm.
Two components are by component one: make polyurethane coating after the stirring of component two=5:1 (weight ratio) proportioning.Spraying this polyurethane coating on the LY12 aluminium alloy of 75mm × 150mm × 2mm, dry 7 days under room temperature, build is 40 ± 5 μm.
The result of neutral salt spray test is in Table 1.As can be seen from Table 1, the salt spray resistance of the coating sample that embodiment 1～4 is prepared with nano compound polyurethane aircraft coating is substantially better than the conventional polyurethanes coating sample not having nano slurry, organic inhibitor, rust resisting pigment of comparative example 1.It addition, from embodiment compared with corresponding comparative example, corrosion extension width in cut place substantially narrows, it was shown that polyurethane aircraft coating significantly increases the corrosion resistance of coating.
Table 1
| Salt fog resistance (level) | Cut place corrosion extension Breadth Maximum, mm | |
| Embodiment 1 | 1 | 0.4 |
| Embodiment 2 | 0 | 0.6 |
| Embodiment 3 | 1 | 0.5 |
| Embodiment 4 | 0 | 0.5 |
| Comparative example 1 | 2 | 2.8 |
Embodiment is it is shown that the present invention proposes to adopt Novel composite nano slurry, rust resisting pigment, compound organic inhibitor and water etc. to prepare nano compound polyurethane aircraft coating so that nano-powder material stably dispersing in coating, and improves the corrosion resistance of coating.Owing to using Chrome-free rust resisting pigment, the coating of preparation is conducive to environmental conservation.It addition, this paint compatibility is good, stable chemical performance, excellent storage stability, not easily sink to the bottom.
Claims (5)
1. a nano compound polyurethane aircraft coating, it is characterised in that be made up of component one and component two, wherein:
(1) counting by weight, component one is made up of following components and content:
Water based acrylic resin 60-80 part；
Nano slurry 5-10 part；Nano slurry is made up of nano titanium oxide, nano silicon, deionized water, silane coupler, PAMC dispersant and waterborne polyurethane resin, wherein: nano titanium oxide, nano silicon, deionized water weight ratio be (10～20): (40～50): (30～50), silane coupler accounts for the 2～4% of above-mentioned nanoparticle gross weight, polyacrylamide dispersant accounts for the 3～5% of above-mentioned nanoparticle gross weight, waterborne polyurethane resin accounts for the 5～8% of above-mentioned nanoparticle gross weight；
Coloring pigment 1-3 part；
Organic inhibitor 8-10 part, organic inhibitor is the compositions of laruate, palmitate, stearate and cinnamate；
Rust resisting pigment 10-15 part, rust resisting pigment is polyaniline modified micaceous iron oxide or polyaniline-modified glass flakes；
Filler 1-5 part；
Auxiliary agent 1-3 part；
Deionized water 20-30 part；
(2) counting by weight, component two is made up of following components and content:
Water-based isocyanate firming agent 70-80 part；
Deionized water 20-30 part；
The weight proportion of component one and component two is (100:10)～(100:30)；
Laruate be sodium laurate, potassium laurate one or both, palmitate be sodium palmitate, potassium palmitate one or both, stearate be sodium stearate, potassium stearate one or both, cinnamate be Fortificar, potassium cinnamate one or both；
The structure of polyaniline modified micaceous iron oxide is laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is micaceous iron oxide；The thickness of clad is 10～20 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 80～90wt%, and phytic acid accounts for 10～20wt%；
The structure of polyaniline-modified glass flakes, for being laminated structure, consists of: surface coating layer is polyaniline and phytic acid, and inside is glass flake；The thickness of clad is 10～30 μm, and in clad, polyaniline and phytic acid are uniformly distributed, and polyaniline accounts for 80～90wt%, and phytic acid accounts for 10～20wt%.
2. the preparation method of the nano compound polyurethane aircraft coating described in a claim 1, it is characterised in that operation as follows:
1) water based acrylic resin, deionized water, nano slurry, auxiliary agent are added in a reservoir, high speed dispersor is utilized to disperse 5～10 minutes at 400～500rpm, add coloring pigment, organic inhibitor, rust resisting pigment and filler, disperse 20～30 minutes through 500～1000rpm；
2) above-mentioned material being carried out sand milling, the sand milling time is 1～4 hour, behind test fineness≤40 μm, and discharging, filter, packaging, prepare into component one；
3) water-based isocyanate firming agent is joined in stirred tank, add deionized water dilution, utilize high speed dispersor to disperse 5～20 minutes at 400～500rpm, discharging after filtration, packaging, prepare into component two；
4) adding in component one by component two, after stirring, spraying, brushing or dip-coating are in substrate surface, room temperature or the formation nano compound polyurethane aviation coating that is heating and curing.
3. the preparation method of the nano compound polyurethane aircraft coating described in claim 2, it is characterised in that when rust resisting pigment is polyaniline modified micaceous iron oxide, the preparation method of polyaniline modified micaceous iron oxide is as follows:
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein, phosphoric acid is 0.01～5 mol/L, and phytic acid is 0.01～1 mol/L；
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.01～1 mol/L, continues to stir；Take phosphoric acid and phytic acid, aniline mixed aqueous solution 500mL, add 200～1000 order micaceous iron oxides of 5～1000g, and after stirring, be pre-chilled to 0～10 DEG C；
The aqueous solution of (c) preparation oxidant: in solution, the concentration of oxidant is 0.05～5 mol/L, and the aqueous solution of oxidant is pre-chilled to 0～10 DEG C；Oxidant is one or more mixture of Ammonium persulfate., hydrogen peroxide, potassium peroxydisulfate, benzoyl peroxide；
D solution prepared for 500mL step (c) is add containing in the phosphoric acid prepared for 500mL step (b) of micaceous iron oxide and phytic acid, aniline mixed aqueous solution in 10～30 minutes in the time by (), react 1～8 hour at 0～10 DEG C, centrifugal, with distilled water wash, 80～100 DEG C after dry 1～5 hour, with mortar grinder, and sieve, obtain the micaceous iron oxide that bottle-green 200～1000 order electrically conductive polyanilines are modified.
4. the preparation method of the nano compound polyurethane aircraft coating described in claim 2, it is characterised in that when rust resisting pigment is polyaniline-modified glass flakes, the preparation method of polyaniline-modified glass flakes is as follows:
(a) preparation phosphoric acid and phytic acid mixed aqueous solution: wherein phosphoric acid is 0.01～5 mol/L, and phytic acid is 0.01～1 mol/L；
B aniline is joined in phosphoric acid and phytic acid mixed aqueous solution by (), mixed concentration of aniline is: 0.01～1 mol/L, continues to stir, take phosphoric acid and phytic acid, aniline mixed aqueous solution 500mL, add the 80-1000 order glass flake of 5～1000g, and stir, be pre-chilled to 0～10 DEG C；
The aqueous solution of (c) preparation oxidant: in solution, the concentration of oxidant is 0.05～5 mol/L, and the aqueous solution of oxidant is pre-chilled to 0～10 DEG C；Oxidant is one or more mixture of Ammonium persulfate., hydrogen peroxide, potassium peroxydisulfate, benzoyl peroxide, ferric chloride, potassium dichromate, potassium permanganate；
(d) by solution prepared for 500mL step (c) the time be add in 10～30 minutes step (b) prepared containing in the 500mL phosphoric acid of glass flake and phytic acid, aniline mixed aqueous solution, react 1～8 hour at 0～10 DEG C, centrifugal, with distilled water wash, 80～100 DEG C after dry 1～5 hour, with mortar grinder, and sieve, obtain the glass flake that bottle-green 80～1000 order electrically conductive polyanilines process.
5. the preparation method of the nano compound polyurethane aircraft coating described in claim 2, it is characterised in that the preparation method of nano slurry is as follows:
Nano titanium oxide and nano silicon are added in deionized water, carries out ultrasound wave and disperse 20～30 minutes, temperature T=30～40 DEG C；It is separately added into silane coupler, PAMC dispersant and waterborne polyurethane resin more wherein and carries out ultrasound wave dispersion 1～2 hour, temperature T=50～60 DEG C；Last in (1～3) × 104It is centrifuged 2～3 times under rev/min, centrifugal 0.5～2 hour every time, prepares nano slurry.
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| CN115261842A (en) * | 2022-07-15 | 2022-11-01 | 攀钢集团攀枝花钢铁研究院有限公司 | Organic composite passivation treating fluid for hot-dip galvanized sheet and use method thereof |
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